Aqueous phase preparation method of ZnSe/ZnS core-shell structure quantum dots

A water-phase preparation and core-shell structure technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of ZnSe quantum dots such as long time-consuming, inability to apply biomarkers, and tailing of fluorescence emission peaks, and achieve low price and source Rich, good biocompatible effect

Inactive Publication Date: 2011-07-20
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for a long time, the ZnSe quantum dots prepared by the hydrothermal method using simple mercapto compounds as ligands take a long time, have large surface defects, obvious tailing phenomenon in the fluorescence emission peak, and the fluorescence quantum yield is relatively low. Low, cannot be applied to biomarkers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Below by embodiment, further illustrate outstanding feature of the present invention, only in order to illustrate the present invention and in no way limit the present invention.

[0022] A ZnSe / ZnS core-shell quantum dot, which consists of: selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 O), reduced glutathione (GSH), and the rest are aqueous solutions.

[0023] In the described ZnSe / ZnS core-shell structure quantum dots, selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 The molar ratios of O) and reduced glutathione (GSH) were 1 / 15~1 / 10:1:1.6~1.8, and heated at 95°C for 45~60min.

[0024] The pH value of the solution is 10-11.

[0025] A water phase preparation method of ZnSe / ZnS core-shell structure quantum dots, the steps are:

[0026] 1. Weigh 0.03006g potassium borohydride (KBH 4 ) and 0.00789g of selenium powder (Se) in a stoppered test tube, add 2mL of high-purity water to it, and plug the stopper. React at -3, or -4, or -5°C for 0.5, or 1, or 1.5h to o...

Embodiment 2

[0031] A ZnSe / ZnS core-shell quantum dot, which consists of: selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 O), reduced glutathione (GSH), and the rest are aqueous solutions.

[0032] In the described ZnSe / ZnS core-shell structure quantum dots, selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 The molar ratios of O) and reduced glutathione (GSH) were 1 / 15~1 / 10:1:1.6~1.8, and heated at 95°C for 45~60min.

[0033] The pH value of the solution is 10.5

[0034] A water phase preparation method of ZnSe / ZnS core-shell structure quantum dots, the steps are:

[0035] 1. Weigh 0.03006g potassium borohydride (KBH 4 ) and 0.00789g of selenium powder (Se) in a stoppered test tube, add 2mL of high-purity water to it, plug the stopper, and react at -4°C for 0.5, or 1, or 1.5h to obtain a colorless transparent liquid, which is 0.05 mol / L of potassium selenide (KH 4 Se).

[0036] 2. Weigh 0.10975 zinc acetate (Zn(Ac) 2 2H 2 O) crystal and 0.24586g reduced glutathione (GSH), disso...

Embodiment 3

[0041] 1. Weigh 0.03006g potassium borohydride (KBH 4 ) and 0.00789g of selenium powder (Se) in a stoppered test tube, add 2mL of high-purity water to it, plug the stopper, and react at -4°C for 0.5, or 1, or 1.5h to obtain a colorless transparent liquid, which is 0.05 mol / L of potassium selenide (KH 4 Se);

[0042] 2. Weigh 0.10975 zinc acetate (Zn(Ac) 2 2H 2 O) crystal and 0.24586g reduced glutathione (GSH), dissolve in 200mL oxygen-free high-purity water.

[0043] 3. Add 1mL of 0.05mol / L potassium selenide (KH 4 Se), adjust the solution pH value to 10 or 10.5 or 11 with the sodium hydroxide (NaOH) of 5mol / L, treat that it mixes completely, potassium selenium hydride (KH 4 Se), zinc acetate (Zn(Ac) 2 2H 2 O), the molar ratios of reduced glutathione (GSH) were 1 / 10:1:1.6, respectively.

[0044] 4. Afterwards, 50ml per can was divided into polytetrafluoroethylene digestion tanks, and microwaved at 95°C for 60 minutes to prepare ZnSe / ZnS core-shell structure quantum dot...

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Abstract

The invention discloses an aqueous phase preparation method of ZnSe/ZnS core-shell structure quantum dots. The aqueous phase preparation method comprises the following steps of: A, preparing KH4Te solution, namely preparing by reducing tellurium powder with sodium borohydride; B, respectively weighing potassium borohydride and selenium powder and adding into a test tube with a stopper, adding high purity water into the test tube, and plugging the stopper to obtain colorless and transparent liquid, namely selenium potassium hydride; C, weighing zinc acetate crystals and reduced glutathione respectively, and dissolving in anaerobic high purity water; D, adding the selenium potassium hydride under the condition of stirring at the speed of 150 to 300 revolutions/min and continuously introducing high purity argon, adjusting a pH value of the solution by using sodium hydroxide solution, and mixing; and E, packaging in a polytetrafluoroethylene digestion tank, and performing microwave heating, wherein a molar ratio of KH4Se to Zn(Ac)2.2H2O to the reduced glutathione is (1/15-1/10):1:(1.6-1.8). The preparation process of the quantum dots is easy, and is high in biocompatibility and fluorescent quantum yield, heavy metal ion toxicity is avoided, fluorescence labeling can be performed on organisms without the aftertreatment process, and process parameters are easy to control.

Description

technical field [0001] The invention relates to novel fluorescent nanometer materials, and more specifically relates to a water-phase preparation method of ZnSe / ZnS core-shell structure quantum dots, which can be used for biological labeling and detection. Background technique [0002] ZnSe quantum dots as green quantum dots can overcome the limitation of quantum dots with heavy metal ion toxicity. However, for a long time, the ZnSe quantum dots prepared by the hydrothermal method using simple mercapto compounds as ligands take a long time, have large surface defects, obvious tailing phenomenon in the fluorescence emission peak, and the fluorescence quantum yield is relatively low. Low, cannot be applied to biomarkers. Therefore, using reduced glutathione as a ligand to prepare quantum dots by microwave heating can shorten the synthesis time, and form a layer of ZnS shell outside the core structure of ZnSe quantum dots, effectively reducing the Surface defects, and increas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/88
Inventor 周培疆陈驰丁玲何振宇
Owner WUHAN UNIV
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